气相和颗粒物中邻苯二甲酸酯的采样与检测技术

对邻苯二甲酸酯的性质及其在环境空气中的存在状态、样品采集技术与分析方法进行了综述,侧重介绍了样品的采集、净化、采样效率和采样与分析全过程的质量控制。     

呼和浩特市大气中酞酸酯的初步研究

通过对呼和浩特市不同功能区和不同季度的大气中酞酸酯污染物的采样监测调查，证实了酞酯不仅存在于大气中，且浓度比较高，为５３１ｎｇ／ｍ＾３，是草原地区背景值（１０－３３ｎｇ／ｍ＾３）的１６倍以上。根据调查表明，不同功能区中大气中酞酸酯（ＤＮＢＰ和ＤＥＨＰ）的浓度差异较大；相同功能区的不同季节，酞酸酯浓度也存在较大差异，但酞酸酯浓度与大气颗粒物呈现出良好的相关性，冬、夏季的相关系数分别为０．９７１和０．     

Determination of 15 phthalate esters in air by gas-phase and particle-phase simultaneous sampling

Based on previous research, the sampling and analysis methods for phthalate esters (PAEs) were improved by increasing the sampling flow of indoor air from 1 to 4 L/min, shortening the sampling duration from 8 to 2 hr. Meanwhile, through the optimization of chromatographic conditions, the concentrations of 9 additional PAE pollutants in indoor air were measured. The optimized chromatographic conditions required a similar amount of time for analysis as before, but gave high responsivity, the capability of simultaneously distinguishing 15 kinds of PAEs, and a high level of discrimination between individual sample peaks, as well as stable peak generation. The recovery rate of all gas-phase and particle-phase samples of the 15 kinds of PAEs ranged from 91.26% to 109.42%, meeting the quantitative analysis requirements for indoor and outdoor air sampling and analysis. For the first time, investigation of the concentration levels as well as characteristics of 15 kinds of PAEs in the indoor air from four different traffic micro-environments (private vehicles, busses, taxis and subways) was carried out, along with validation of the optimized sampling and analytical method. The results show that all the 9 additional PAEs could be detected at relatively high pollution levels in the indoor air from the four traffic micro-environments. As none of the pollution levels of the 15 kinds of PAEs in the indoor air from the 4 traffic micro-environments should be neglected, it is of great significance to increase the types of PAEs able to be detected in indoor air.     

液相色谱法测定环境空气中酞酸酯类

制作了半挥发性有机物中流量采样装置,使用超细玻璃纤维滤膜采样,反相液相色谱法测定环境空气中酞酸酯类,并对样品净化方式、目标化合物在气相和颗粒物上的分布规律及采样器的捕集效率进行了试验.方法在0.50 mg/L～50.0 mg/L之间线性关系良好,当浓缩体积为1.0 mL、采样体积为144 m3时,目标化合物的检出限为0.4×10-3 μg/m3～6.0×10-3 μg/m3;当采样体积为6 m3时,检出限为0.008 μg/m3～0.145 μg/m3.     

固相萃取- GC/MS法测定水中邻苯二甲酸酯类

采用固相萃取-GC／MS法测定水中6种邻苯二甲酸酯类有机污染物,比较了不同固相萃取柱对萃取效果的影响,优化了水样pH值、水样流量、穿透体积、洗脱溶剂、洗脱剂体积、洗脱流量等萃取条件。方法在0．050μg/L-800μg/L范围内线性良好,检出限为0．008μg/L～0．03μg／L,标准溶液测定的RSD≤10．5％,实际水样加标回收率为80．0％-100％。     

北京公园水体中邻苯二甲酸酯类物质的测定及其分布特征

为了正确评估北京市公园水体受PAEs污染的程度,采集了北京11个公园湖水的水样,采用固相萃取-气相色谱联用技术检测了其中六种邻苯二甲酸酯类物质(PAEs)的含量,该方法加标回收率在73%～89.3%,RSD为5.9%～18.1%,检出限在0.40～4.58mg/L。实验结果为北京公园水体中总PAEs浓度在6.4～138.1μg/L,平均值为27.9μg/L,证明北京公园水体受到不同程度的PAEs污染,主要的污染物为邻苯二甲酸二丁酯(DBP)和邻苯二甲酸双(2-乙基己基)酯(DEHP),其中东南部以及西北部的公园污染较严重。分析了PAEs在公园湖水底泥中和水体中的分布特征,结果显示,PAEs在湖水底泥中的含量明显大于在水体中的含量。     

土壤中酞酸酯类化合物监测方法的质量控制研究

从监测结果控制的角度对近10年的土壤中PAEs监测方法进行了探讨,重点比较了索氏萃取柱净化GC/MS、微波萃取柱净化GC、加速溶剂萃取柱净化GC/MS和加速溶剂萃取GPCGC/MS方法的检出限、精密度和准确度。旨在为中国土壤监测方法的建立提供基础支撑,为开展质量控制工作提供评价依据。     

Phthalate exposure in pregnant women and their children in central Taiwan

Phthalate exposure was found to be associated with endocrine disruption, respiratory effects, reproductive and developmental toxicity. The intensive use of plastics may be increasing the exposure to phthalates in Taiwanese population, particularly for young children.We studied phthalate metabolites in pregnant women and their newborns in a prospective cohort from a medical center in Central Taiwan. One hundred maternal urine samples and 30 paired cord blood and milk samples were randomly selected from all of participants (430 pregnant women). Eleven phthalate metabolites (MEHP, 5OH-MEHP, 2cx-MEHP, 5cx-MEPP, 5oxo-MEHP, MiBP, MnBP, MBzP, OH-MiNP, oxo-MiNP, and cx-MiNP) representing the exposure to five commonly used phthalates (DEHP, di-isobutyl phthalate (DiBP), DnBP, BBP, DiNP) were measured in urine of pregnant women, cord serum and breast milk after delivery, and in urine of their children. Exposure was estimated with excretion factors and correlation among metabolites of the same parent compound. Thirty and 59 urinary samples from 2 and 5 years-old children were randomly selected from 185 children successfully followed.Total urinary phthalate metabolite concentration (geometric mean, μg L⁻¹) was found to be higher in 2-years-olds (398.6) and 5-years-olds (333.7) than pregnant women (205.2). Metabolites in urine are mainly from DEHP. The proportion of DiNP metabolites was higher in children urine (4.39 and 8.31%, ages 2 and 5) than in adults (0.83%) (p < 0.01). Compared to urinary levels, phthalate metabolite levels are low in cord blood (37.45) and milk (14.90). DEHP metabolite levels in women’s urine and their corresponding cord blood are significantly correlated. Compared to other populations in the world, DEHP derived metabolites in maternal urine were higher, while phthalate metabolite levels in milk and cord blood were similar. The level of phthalate metabolites in milk and cord blood were comparable to those found in other populations. Further studies of health effects related to DEHP and DiNP exposure are necessary for the children.     

Pollution levels and characteristics of phthalate esters in indoor air of offices

The pollution status and characteristics of PAEs (phthalate esters) were investigated in indoor air of offices, and PAEs of both gas-phase and particulate-phase were detected in all the samples. The concentration (sum of the gas phase and the particulate phase) was 4748.24 ng/m³, ranging between 3070.09 and 6700.14 ng/m³. Diethyl phthalate, dibutyl phthalate, and di(2-ethylhexyl) phthalate were the most abundant compounds, together accounting for 70% of the Σ6PAEs. Dividing the particulate-phase PAEs into four size ranges (<2.5, 2.5-5, 5-10, >10 μm), the result indicated that PAEs in PM_2.5 were the most abundant, with the proportion of 72.64%. In addition, the PAE concentration in PM_2.5 correlated significantly with the total particulate-phase PAEs (R² = 0.85). Thus, the amount of PAEs in PM_2.5 can be estimated from the total amount of particulate-phase PAEs using this proportion. In a comparison between the offices and a newly decorated study room, it was found that pollution characteristics were similar between these two places. Thus, it is implied that the PAE concentration decreased by 50% 2 yr after decorating.     

Pollution levels and characteristics of phthalate esters in indoor air of offices

The pollution status and characteristics of PAEs(phthalate esters) were investigated in indoor air of offices, and PAEs of both gas-phase and particulate-phase were detected in all the samples. The concentration(sum of the gas phase and the particulate phase) was4748.24 ng/m3, ranging between 3070.09 and 6700.14 ng/m3. Diethyl phthalate, dibutyl phthalate, and di(2-ethylhexyl) phthalate were the most abundant compounds, together accounting for 70% of the ∑ 6PAEs. Dividing the particulate-phase PAEs into four size ranges( 2.5, 2.5–5, 5–10, 10 μm), the result indicated that PAEs in PM2.5were the most abundant,with the proportion of 72.64%. In addition, the PAE concentration in PM2.5correlated significantly with the total particulate-phase PAEs(R2= 0.85). Thus, the amount of PAEs in PM2.5can be estimated from the total amount of particulate-phase PAEs using this proportion. In a comparison between the offices and a newly decorated study room, it was found that pollution characteristics were similar between these two places. Thus, it is implied that the PAE concentration decreased by 50% 2 yr after decorating.